Pillared Layered Structures Based upon M(III) Ethylene Diphosphonates: The Synthesis and Crystal Structures of M<sup>III</sup>(H<sub>2</sub>O)(HO<sub>3</sub>P(CH<sub>2</sub>)<sub>2</sub>PO<sub>3</sub>) (M = Fe, Al, Ga)
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A three-dimensional iron(III) diphosphonate, FeIII(H2O)(HO3P(CH2)2PO3), I, has been synthesized hydrothermally and characterized by single-crystal X-ray diffraction. The compound crystallizes in the orthorhombic space group Pbca (no. 61) where a = 9.739(5) Å, b = 9.498(5) Å, c = 15.940(8) Å, V = 1474.4(1) Å3, Z = 8, and R1 = 0.0380. The structure consists of inorganic sheets pillared by the 1,2-ethylenediphosphonate groups. The sheets are composed of Fe(H2O)O5 octahedra connected through PO3C tetrahedra. The corresponding isostructural aluminum (II) and gallium (III) compounds were also synthesized and indexed: II, a = 9.534(1) Å, b = 9.255(2) Å, c = 15.724(1) Å, V = 1387.5(1) Å3; III, a = 9.670(1) Å, b = 9.357(2) Å, c = 15.862(4) Å, V = 1435.4(1) Å3.



